反応 #2196

ord-27d91eecd20e450da1b8e17f791b0eaa

反応方程式

CSCc1ccc(C(=O)c2ccc(Cl)cc2)cc1
4-chloro-4'-methylthiomethylbenzophenone
CO
methanol
[Na+].[O-][I+3]([O-])([O-])[O-]
Sodium periodate
CS(=O)Cc1ccc(C(=O)c2ccc(Cl)cc2)cc1
desired product
収率 93.0%
CS(=O)Cc1ccc(C(=O)c2ccc(Cl)cc2)cc1
4-Chloro-4'-methylsulfinylmethylbenzophenone
収率 93.0%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas added to this solution
  2. 2
    濃縮The reaction mixture was concentrated
  3. 3
    workup.ADDITIONwater was added
  4. 4
    抽出The mixture was extracted with ethyl acetate
  5. 5
    洗浄The ethyl acetate layer was washed with water
  6. 6
    乾燥dried over anhydrous magnesium sulfate
  7. 7
    workup.DISTILLATIONEthyl acetate was distilled off under reduced pressure
  8. 8
    洗浄The residual solid was washed with n-hexane

実験手順

4-chloro-4'-methylthiomethylbenzophenone (4.2 g) was added to methanol (150 ml). Sodium periodate (3.6 g) dissolved in water (20 ml), was added to this solution, and the mixture was stirred for 16 hours at room temperature. The reaction mixture was concentrated, and water was added thereto. The mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with water and then dried over anhydrous magnesium sulfate. Ethyl acetate was distilled off under reduced pressure. The residual solid was washed with n-hexane to obtain the desired product (4.1 g, melting point: 116° to 118° C., yield: 93%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05728699uspto-grants-1998_03